反应详情

温度

70 °C

300 mg (1.21 mmol) of 1-allyl-4-(6-nitropyridin-3-yl)piperazine from Example 15.1 were dissolved in 20 ml of methanol, after which 2.18 g (9.67 mmol) of tin(II) chloride dihydrate were added and the mixture was stirred at 70° C. for 2 hours. After the solvent had been evaporated down to dryness, the resulting residue was treated with water and this mixture was made alkaline using a dilute aqueous solution of sodium hydroxide and extracted with ethyl acetate. The solid which had precipitated out was filtered off with suction. The phases were then separated and the aqueous phase was extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and evaporated down to dryness, with 183 mg (69% of theory) of the title compound being obtained.

1. customAfter the solvent had been evaporated down to dryness
2. additionthe resulting residue was treated with water
3. extractionextracted with ethyl acetate
4. customThe solid which had precipitated out
5. filtrationwas filtered off with suction
6. customThe phases were then separated
7. extractionthe aqueous phase was extracted three times with ethyl acetate
8. dry with materialThe combined organic phases were dried over sodium sulfate
9. filtrationfiltered
10. customevaporated down to dryness, with 183 mg (69% of theory) of the title compound
11. custombeing obtained